Methanol → HCID 69156547, compound

Participants

Reaction Conditions

Reaction Steps

A 12 ml portion of 4 M hydrochloric acid-dioxane solution was added to a mixture of 580 mg of tert-butyl ester of 3-[2-(2-aminoethylamino)-5-carbamoylpyrimidin-4-ylamino]benzoic acid with 6 ml of methanol and 6 ml of water and stirred at 80° C. for 1 hour. The organic solvent was evaporated from the reaction mixture under a reduced pressure, and the thus formed precipitate was collected by filtration. After adding methanol and water, the mixture was heated. The insoluble matter was removed by filtration and then the mother liquid was concentrated under a reduced pressure. By recrystallizing the resulting residue from a mixed solvent of methanol and water, 59 mg of 3-[2-(2-aminoethylamino)-5-carbamoylpyrimidin-4-ylamino]benzoic acid dihydrochloride was obtained (colorless crystals).

Provenance & Evidence